ABUNDANCE AND DISTRIBUTION OF CERTAIN
ELEMENTS IN SPHENE
by
EDWIN ROBERT ROSE
SUBMITTED IN PARTIAL FULFILLMENT
OF THE REQUIREMENTS FOR THE
WEc
DEGREE OF MASTER OF
SCIENCE
~QjX~w
at the
MASSACEUSETTS INSTITUTE OF
TECHNOLOGY
August, 1959
Signature of Author
t.....................................
Departmenyof Geology and Gp6phytes, August 22, 1959
Certified by ...
Thesis Supervisor
Accepted by -rre.06.......................l
Chairman, Departmental Cowmittee on Graduate Students
4
ABTRACT
AfUNDANCE AND DISTRIBUTION OF C)RTAIN SLMTS IN SPHESN
by Edwin Robert Rose
Submitted to the Department of Geology and Geophysics
August 24, 1959 in partial fulfillment of the requirementa
for the degree of Master of Science
The trace element content of accessory aphene from granitio rocks was
investigated to determine if genetic similarity between igneous rocks can
be detected by such means. This study also supplies considerable data on
the trace element contents of spheneso
Analyses were made using a grating spectrograph on a Wadsworth mounting. Quantitative determinations were made for iron, chromium, zirconium,
neodymium, lanthanum, cerium, samarium, gadolinium, scandium, vanadium,
yttrium and tungsten in twenty-Uthree samples from northeastern North Amer.iea. Semi-quantitative estimates were made for aluminum and strontium
whenever present.
A standard was prepared from one of the aphene samples. This standard
was then used as a "measuring stick" in the determinations of the analysis
elements in the remaining twenty-two samples. The original concentrations
of the analysis elements in the standard was determined by use of the addition procedure. In connection with the addition plots, use was made of a
ratio of the intensity of each analysis element to either oalcium or titaninm; usually calcium. This ratioing of intensities improved the addition
plots in most cases, making it easier to determine the original conoentretions of the analysis elements in the standard. It is estimated that the
error involved in some of the determinations may vary from about ten percent to perhaps as much as twenty percent. Different element s will have
different errors.
It was found that lanthanum, cerium and neodymium were geohemically
coherent as were samarium and gadolinium. Cerium and lanthanum showed an
inverse relationship to yttrium. Samples highest in chromium seemed to be
lowest in iron. Chromium, soandium and tungsten concentrations were low
in all samples. Iron was always present in high coneentrations, averaging
about 20,000 ppm. The remainder of the analysis elements with an oceasional
exception were present in quantities less than one percent (10,000 ppm).
Manganese, yttrium, and neodymium values generally fell in a range from
3500 to 6000 ppm, Gadolinium, samarium, lanthanum, erium, zireonium and
vanadium values lie for the most part between 1000 and 3500 ppm.
Eleven of the thirteen samples from New England showed signifisant
similarity to one another. This group, containing most of the New Rngland
samples, is distinctly different from the rest of the samples. Similarity
between three samples from Ontario is noted, Analyses of two samples from
Quebee also show a distinct relationship to each other.
The results seem to indicate that trace element conteat of ephene can
be useful in determining the fact of genetic relat ionships between igneous
rock,
Thesis Supervisor: William H. Dennen
Associate Professor of Geology
C0oaNfTS
Aoknowledgments . . . . . . . . . . . . . . . . . . . . . . . . . .
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Introduction
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Selection of Analysis
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Sample Preparation
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Method of Analysis
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Swary of Results and Conclusions
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Addition Plots
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Calibration Curves
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TAaM
Table
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Analysis Lines used in Addition Procedure
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Compounds of Analysis Element a used in
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Concentration of Analysis Alements in Samples
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Determinations of the Elements 'by
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FIGURES
Figure
3
Variation of Arcing Time with Sample Weight . . . . . . .
Fe 4383 A
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Addition Plots for Fe 4260 A
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Map of Sample Localities
Addition Plots for
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GRAPES
Graph
1
2
Concentration Plots for Iron, Manganese and Chromium
Concentration Plot for Zirconium . . . , . .
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Concentration Plot for Yttrium
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Concentration Plot for Neodymiui
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Concentration Plot for Samarium
Concentration Plot for
candium
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Concentration Plot for Cerium a nd Lanthanum
Cone entrat ion Plot for GadoliniuM
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Concentration Plots for Samples 3011 and 3055
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Concentration Plots f or Samples 3014, 3058 and 3071
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Concentration Plots for Samples 3080 and 3139
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Concentration Plots for Samples 3051, 3080 and 3061
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Concentration Plots for Samples 3082, 3063 and 3079
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Concentration Plots for Sanmples 3081) 3082 and 3485
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Concentration Plots for Samples
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Concentration Plots for Samples 3084 and 3085
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Conoentration Plot for Sample 2C93
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Concentration Plot for Sample 3C13 .X . . . . . . .
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Concentration Plot for Sanple 31
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ACKNOWLEDGMENTS
The author expresses his sincere gratitude and appreciation to
Dr. William H. Dennen, thesis supervisor, for his suggestion of the thesis
possibility and for continued suggestions and advice during the course of
the entire thesis investigation.
INTRODUCTION
Purpose
The purpose of this thesis is to investigate the possibility that the
trace element distributions and variation in sphene might be used as a
means of establishing or recognizing genetic similarity or dissimilarity
between granitic rocks.
To date little trace element analysis of sphene
has been done and thus little is known concerning the trace element content of sphene.
This investigation will furnish considerable data on the
abundance and distribution of certain trace elements in this mineral.
The usefulness of trace element distribution as a possible means to
group and separate igneous rocks of similar and different histories is
based on the assumption that elements present in trace quantities do not
effect the cooling of the magma.
It is important that one choose elements
accepted into the ephene structure that have varing concentrations in different magnas and that this variation of original concentration be reflected by the relative proportions of the same elements in the sphenes.
Sphene was chosen as the analysis mineral for this investigation for
two main reasons.
First, considering its formula CaTi(Si0 4 )0, and the
previous work done (to be covered later), it appeared that the mineral
would furnish ample opportunity for substitution of trace elements in its
structure.
This is quite important since in an investigation of this
type it is desirable to have detectable amounts of several trace elements
present in order to establish some understanding of the significance of
the results.
It is impractical to attempt to make determinations of trace
elements in a mineral which admits non-formulary constituents only in
quantities below the detection limits of the method used#
It is also
useless to investigate a mineral which is, so to speak, a trash bin for
a great number of elements which enter its structure without any selection,
and in a great variety of concentrations.
A second reason for choosing sphene as the analysis mineral was the
availability of over twenty aphene samples separated from granitic rocks.
These samplea were from rooks used in a program of radioactive age studies
in the M.I.T. Department of Geology and Geophysics.
In connection with
this program, granitic rocks from northeastern North America were collected,
crushed, and ortain minerals of which sphene was one, were separated
(Hurley and Fairbairn, 1957).
Of course, the fundamental consideration
behind this availability of sphene, is the widespread occurrence of sphene
as an accessory mineral in granitic rooks.
Previo s Work
Review of the literature showed that little work has been done on the
trace element constituents and their quantities in sphenes.
Fersman (1926) reports analysis of a sphene from a nephelite syenite.
This analysis shows 1700 ppm of cerium and yttrium oxides and about 1200
ppm of iron oxides both ferrous and ferrio.
tities of magnesium, sodium and potassium.
(1937),
Also reported are trace quanAnother article by Forsman
though not seen by the author in supposed to include some data on
sphenes.
Bray (1942),
states "sphenes are notable for their high rare-
earth content, as well as high aluminum, iron, manganese, chromium and
vanadium."
The work which Bray did on the sphenes was qualitative and
thus one cannot estimate what "high" means.
Bray himself points out that
this is a relative term for each element and what is high for one element
may be low for another.
In a study of four sphenes, one of which was the rare-earth-rtch
variety, keilhauite, Prince (1938) reports from about one to not quite
four percent iron oxide.
In each of the "normal" aphenes he also found
about six percent aluminum oxide and several hundredths of a percent of
nanganese oxide was reported in two of the sataplse.
In the keilhauite
variety, Prince reports 3.58 percent (35,800 ppm) for the total of cerium
and yttrium oxides, about six percent ferrie oxide and over seven percent
of aluminum oxide.
Bahmae (1946) reports quantative analyses of six sphenes, three from
nephelite syenites on the Kola Peninsulb, one from a limestone, one from
a gabbro, both of these from Finland and the sixth specimen from the Urals.
For the rare-earth group of elements he hs values reported for lanthanum,
cerium, praseodymium, neodymium, samarium, gadolinium, dysprosium, erbium,
ytterbium and yttrium oxides.
Values for these oxides range from a trace
to about 1200 ppm, with neodymium, lanthanum, cerium and yttrium running
in quantities several times larger than the concentrations of 100 to 200
ppm for the other rare-earth oxides.
form by Sahama include:
Other elements determined in oxide
tantalum, vanadium, aluminum, iron, ebromium,
magnesium, zirconium, strontium, barium, manganese and niobium.
oxide values vary from 300 ppm to over 15,000 ppm.
are 300 ppm or less.
about 800 ppm.
Niobium
Tantalum oxide values
The values for vanadium oxide are of the order of
Ferrous iron oxide values lie in the neighborhood of 2,000
ppm, zirconium oxide values average about 600 ppm, strontium varies highly,
from 40 to 4,400 ppm, while barium oxide varies from 50 to 500 ppm.
Niobium, tantalum, vanadium, iron, zirconium, strontium and barium were
found in all six samples.
Values for aluminum oxide are reported for only
three of the samples and very from 500 to about 4400 ppm.
values are reported for two samples with an
Chromium oxide
average value of 150 ppm.
Other elements reported are magnesium, manganese, sodium and potassium.
Of all these elements only vanadium, chromium and zirconium were analysed
for by spectrochemical techniques.
Sahama (1946) also included an analysis of another aupposed
sphene.
This supposed s7hene contains about 9600 ppm of yttrium oxide, 1900 ppm
of cerium oxide.
These values are considerable larger than those for
any of the other specimens, and this sphene is likewise much higher in
tantalum and iron than any of the other analyses. The total iron oxide
value is reported as 26,000 ppm.
According to Sahama sphene can be used
as an indicator of the bulk composition of the rare-earth elements in
rooks.
In their book, Goehemistry, Rankama and Sahama mention reports of
europium in aphene up to 340 ppm and that it may contain up to several
percent of columbium oxide.
They feel that the yttrium rare-earths are
characteristic of granites, while the cerium rare-earths usually seem to
be enriched in nepheline syanites.
It is also pointed out that aphene is
one of the main seats of radio-activity in igneous rocks.
Coluabium is reported in quantities from 1,000 to 10,000 ppm in aphones
analysed by Jaffe
(1947),
spectrographic methods.
yaffe investigated sixteen sphone samples using
He found iron, aluminum, and fluorine in all
samples and columbium in about half.
Goldsebmidt (1954) notes a sphene variety containing about ten percent
tin dioxide.
He also mentions that the calcium in $phone is frequently re-
placed in part by yttrium, the rare-earths, uranium and thorium and that
one to two percent niobium is found in some sphenes replacing the titanium.
In twenty-four sphene samples, sixteen of which were also used by the
author, Hurley and Fairbairn (1957) determined uranium and thorium
ooncentrations. The average thorium ooncentration was 540 ppm and the
uranium content averaged near 300 ppm.
The minerals ziroon, apatite and
epidote from some of the same rock samples were also analysed for uranim
and thorium.
It was found that the sphenes contained more uranium and
thorium thian apatite and epidote, but less uranium and thorium than
zircon,
Molybdenwa concentretions ranging from 34 to 400 ppm have been reported by rabinovich and associates (1958).
Of the minerals they analysed,
aphones had the largest molybdenum oontent.
The highest values were from
sphenes obtainod from areas near molybdenum mines.
was spectrographic.
The method of analysis
Selection of AnAlysis
lemeuts and Wines
It in necessary in choosing analysis elements to pick elements which
might be expected to be present at least fairly commonly in detectable
quantitias in wphenes.
The selection of onalysis elenents in this work
was done using three primary guides.
One was the consideration of which
trace aleaents ware of suitable size to substitute for one of the major
elements.
The second guide was information available from previous work,
Thio gUide however, was only a rough general guide.
The third guide was
the qualitativc analyis of sphone 3085, the standard.
irportant
step in deciding on the analysis elements.
This was the mst
It was noticed in
the study of the previous work that while the widespread occurrence of
rare-earths in sphenes was noted in most cases, only in the case of Sahama
(1946) was there any major breakdown into the individual slements,
On examination of the spectra of aphene 3085 numerous rare-earth
lines were identified.
These included lines of neodymium, lanthanum,
cerium, gadolinium, samarium, ytterbium, erbium and praseodymium,
The
rare-earth elements chosen for analysis were neodymium, lanthanum, cerium,
gadolinium and saiarium.
The other rare-earths were not chosen as analysis
elements because of the great difficulty in recognizing the individual lines
of the different elements, due to near 'oincidence, primarily with other
rare-earth lines.
These other rare-earth lines were also of very low in-
tensity and thua were assumed to be much more likely to be present only in
quantities near the sensivity limits of the procedure.
It should be noted
here that in the case of gadolinium and samarium, it was still quite difficult to distinguish between the lines of the two elements, since in the
region used they are very close together. In order to furnish some measure
of a check on the correct choice of lines, two lines for smarium and
gadolinium were chosen (see Table 1).
Other elements found to be present in sphene 3085 and chosen as
analysis elements were chromium, iron, manganese, molybdenum, scandium,
vanadium, yttrium, tungsten and zireonium.
Table 1 lists all lines that were measured for use in constructing
the addition plots, their rated intensities as tabulated in the M.I.T.
Wavelength Tables, and the wavelength and intensities of significant
lines that interfere with the particular analysis line.
All lines picked
were the most sensitive lines of each element, which also hed the minimum
of interference from other lines.
Also considered in oases where inter-
ference of some sort seemed unavoidable, was what element was conflicting
with the analysis line.
No analysis line was chosen that had a conflict
with one of the mwjor elements calcium, titanium or silicon.
Every attempt
was alao made not to use analysis lines which conflicted vith a line of
another analysis element.
In esses where this was not entirely possible,
the analysts line was picked whose conflicting line had the lowest intensity rating.
The only elements where it was impossible to avoid choos-
ing enlysis lines with conflicts were
molybdenum and neodyuium.
Molybdenum 3902.93 is the only important molybdenua line in that region
of the spectra investigted.
This line, with an intensity rating of 1000,
had a major interference with iron 3902.94C with an inteaity rating of
500.
An attempt was made to estimate the contribution of the iron to the
intensity of this line, through the use of an intensity ratio of the iron
line to another iron line,
however, it was found on subtracting that
portion of the intensity calculated to be due to the iron line, one was
left with a negative intensity for the molybdenum line for all twenty-three
Teble 1
Analysis Lines used in the Addition Procedure
Line
0
4222
Intensity of
Interfering
Lines
Interfering
Lines
*Intensity
80
1
Cr 4254
5000
Fe 43831
1000
Fe 4260 A
400
Gd 4251,74
E
300
Sm 4251.79
A
200
Gd 4282o09
A
150
Or 4262.13 A
40
Le 4333 A
800
E
500
Mn 4031
Mn 4034l
250
1
1000
Fe 3902.94
E
500
Nd 4303.57 A
100
Fe 4303.58
l
25
So 4246.83 A
80
Nd 4246.88
A
10
A
100
Mo 3902,96
Se 4374.5
S& 4256
A
150
Sm 4329
A
300
Y 4379
l
Y 4374.94
25
40
Zr 4256 1
Nd 4256
200
1
150
Y 4398 A
150
W 4294 A
50
Zr 4239 1
100
,
SM 4374.98
,
*From U.I.T. Wavelength Tebles.
A
200
I
aphene samples.
ele*ents,
As a result molybdenum was dropped from the analysis
Neodymium 430.5'73 also had a conflict *ith an iron line.
contribution of this Iron line was corrected for, as will be described
later, end yielded meeningful results.
The
SPECTRIGRAPHIO PRIPARATION
SaMle Preation
As mentioned earlier, the sphone samples used were available to the
author as minerals separated from granitic rocks.
A list of the samples,
their location, the type of rock from which they came and the estimated
percent contamination is given in Table 2.
These separates were derived
from rock samples of about fifty pounds, which were crushed and concentrated by gravity and magnetic procedures (Fairbairn, 1955),
The author took twenty-three separates and crushed each sample in a
stainless steel mortar. The mortar was cleaned with distilled water after
the crushing of each sample was completed.
That portion of each sample
which passed the two hundred mesh screen and was retained on the three
hundred twenty-five mesh screen was used in the analysis.
The samples
were crushed this fine in order to free the included impurities from the
ephene.
This fraction of the sample then was run through a Frantz iso-
dynamic separator.
Each sample was run through several t imes with varying
amperages and rates of feed in order to remove a maximum amount of contamination.
Of course, some samples showed little or no improvement since
the original contamination was so low.
made under a binocular microscope.
Estimates of contamination were
In all oases more attention was paid
to eliminating opaque and dark impurities than quartz and similar minerals,
since one would expect the opaque mineral to contribute much more heavily
to the elemental contamination than quartz.
The processing of the crushed
sample through the Frantz separator also had the important effect of eliminating any contaminAtion of iron due to the crushing in a steel mortar.
After cleaning the samples an estimate was made of the percent contamination.
This was done by spreading several hundred grains on a small
Table 2
Locality, Rock Type, Other Accessory Minerals, and Uatimated
paercent Contamination of Samples Analysed
Sam- Rook Type
ple
5011
Locality
Other Accessory
Minerals
Granite Leavitt quarry, 2 miles
Biotitemagnetiteapa-
W. of Leominster, Mass.
titetourmaline,ziroon
Hallowell, Maine
Biotite,MUsovit8,ap8.,
3055 Qranite
Zatimated
contamination
6-quartz
3-quartz
fluoritemonazitszir.
3014
Granite
Ourry quarryMaas.,2
. Biotitechlorite,epidote
BS3 of Wrenthem sta.Madf
3058 Wuartz
Granite
John area
On route 198, 2 mi. N.
W05
Biotite,ohlorite,magn.,
ilwn.,epidoteziroon
Granite Route 11, 13.5 mi. Z. of
Mt.
3051
Bio. ,chlor. ,amph.,magn.,
Laurier,
2
Grano- North and of N. Attle-
Chlorite, ilmenite,
boro, Mass.
epidote, zireon_
Granite
Mt
Biotitepyriteapatite,
1Waldo, Maine
tourmaline,
3063
amph.,epd.,fluor.,ziroon
Granite Route 201, 5.5 mi. S. of Chlorite,magnetite,epi0aokman, Maine
dote, apatite, zircon
Granite Hollingsworth & Whit.Rd. Biotite, chlorite, epi6mi.W.from rte. 201, Me.
3079 Granite
Granite
Syenite
Brriefield,Ont.on outKingston Mills, Ont.,
6 mi. N. of Kingston
Amphibole,garnetiagn.,
Biotite, pyrite, magn.,
liln., apatite, zircon
Syenite
Brome Mt., Quebec, on
Biotite,museoviteilmen-
Iron Hill
ite,
Granite
6
2
2
Ont.
Road
3-quartz
zircon
Granite
3069 Tingusite St. Josef's Blvd.,
3084
and quartz
9-($ quartz
i dark min.)
0
tite, zircon
3485 Alaskitio Hope Lake, Kenora Dist.,
3067
4-dark min.
dote, apatite, ziroon
skirts of Kingston, Ont. apatite, tour.,
3082
3-quartz
On rte. 1, 1 mile S. of Chlorite, epidote, aps-
(rapakin) yonesboro, Maine
3081
5-quartz
zircon
Moosehead Lake, Maine on Biotite,ohloritexagn.,
route 15
3062
5-dark min,
and quartz
Que.
diorite
3061 Rhyolite
2-quart
ilannepd.tour.fluor.zir.
bit. Desert, Maine
3139
7-quartz
tourmaline, zircon
St. Gideon, Cue.-Lake
St.
3080
quartz
Sprucehead Island, Maine Biotiteepidote,apatite,
sonzonite
3071 Granite
max. 9-
apatitefluorite,ziroon
apatite,
4-quartz
zircon
Amphibole, magnetite,
Montreal Bast
apatite
Gaspe Nat'l. Park hiway
Chlorite, magnetite,
2-quartz
4-quartz
Porphyy 7 mi. S.of Gaspesie,Quel tourmaline, zircon
3085
Granite W. and Mountainville,
Bio.,ohlor.,amph.,pyrex, 0
io magn.,epd., apa., zircon_
2093 Quartz
Dauphine quarry, Birch- Biotite,ohlorite, apa6-pyrite and
Diorite town, Nova Scotia
tite, zircon
quartz
T013 Granite Blanchard quarry, 1$ m1< Biotite, magnetite,
4-dark min.
Deer Is. Quadrangle,
WW. of Uxbridge Sta.ass,
3138
Granite
fine Dn
fluorite, zircon
Rts. 58, 14.1 mi. W. of
12-opaque
Mt. Laurier, Que.
or dk, min,
--------1-____ I
1 lip 1,0
MOMP
grid under a binocular microscope, counting two to three hundred grains,
and recording the number of non-sphene grains in this count.
Due to the
extremely small size of the grains used, it was not possible in the time
available to determine what the impurities were.
That portion of the
impurities that were opaque minerals is listed with the estimates of contamination in Table 2, Quartz wherever discernible has also been noted,
Mixing
All mixing was carried out using a small agate mortar and pestle,
both of which were scrubbed with cleanser and then well rinsed with distilled water before mixing each sample with either carbon or additive
oxides.
In the case of the samples to which oxides of the analysis ele-
ments were added, mixing in the mortar was carried on in the mortar for
at least thirty minutes.
During this time the sample was swept into a
small pile in the center of the mortar at least six times*
This procedure
was followed in order to get a uniform mixing of the additive oxides with
the sphene standard, The rest of the mixings consisted of mixing one part
of the addition sample or pure sphene sample with two parts of carbon by
weight.
The mixing with carbon was carried out for at least five minutes
with at least five coning procedures.
Electrodes
Bach sample was run in duplicate.
It was found in preliminary quali-
tative work that one eighth inch electrodes with a cylindrical cavity one
sixteenth of an inch in diameter and three sixteenths of an inch deep was
the best available size to use for the sample electrodes,
Spectrographic-
ally pure graphite electrodes were used for all samples throughout the
investigation.
The twelve electrodes used for the addition procedure were weighed
before and after loading of the samples.
The variation in the weights of
the samples in these electrodes averaged about give percent.
None of the
other electrodes was weighed.
Phograhic Materials
Kodak 103-0 spectrographic plates were used in all cases.
After
arcing, each plate was put in a developing tank for four and a half minutes at a temperature of twenty degrees centigrade.
Then the plate was
fixed for at least fifteen minutes, usually longer.
Finally, the plate
was washed for at least thirty minutes.
Photometry
Measurement of line and background intensity was done with a Hilger
non-recording miorophotometer.
Measurement of both line and background
was made on all analysis lines.
Spectrogaph
The analysis instrument was a twenty-one foot, 30,000 lines per inch
concave grating speetrograph on a Wadsworth mounting.
a dispersion of about 2.5
A per
millimeter.
This instrument has
The good dispersion of this
instrument was the basis of the choice of this instrument.
The near
coincidence of many of the rare-earth lines requires a large dispersion
in order to get maximum possible separation of the lines of the different
elements.
The region used in this investigation lay from about 3900
1
0
4500 A. A alit width of 0.015 inch and alit height of about 6.0 millimeters was used.
to
Arcing Conditions
All samples were arced to completion using anode excitation at about
seven amperes.
The electrode separation was about seven and a half milli-
meters. One eighth inch spectrographicelly pure graphite electrodes containing the sample were used at the anode.
The counter electrodes used
were three sixteenths inch spectrographically pure carbon rods, sharpened
to a fine point.
Counter electrodes were changed after each sample and
resharpened for later use.
The average completion arcing time was about
one minute and fifty seconds, with a variation of about five percent.
The
variation of arcing time is to some extent related to the amount of sample
arced (see figure 1).
However, this relationship was not determinable.
It undoubtedly depends on many other things also, such as matrix, amperage,
electrode size, etc.
Sector
In order to reduce the intensities of certain lines to the point where
they could be measured quantitatively, a sector was used. An eight step
sector with a factor of one-half per step was used for the addition procedure on sphone 3085 and for three other sphene samples.
A newly prepared
sector with a step factor of one-fourth was found to be more useful, and
was used on all the remaining samples.
This sector had five steps.
What
is meant by a step-factor of one-fourth can be explained as follows:
assuming oonstant intensity over the ontira area of the sector, the first
step allows the passage of all the light, while each succeeding step permits the passage of a quantity of light equal to only one-fourth that
allowed to pass on the preceding step.
SOURES OF ERROR
There are two general types of errors involved in quantitative
spectroehemical analysis.
They are those inherently present in the sample
and equipment used, and those introduced by the analyst.
In the first group are included errors due to contamination of the
samples, development of the plates, non-linear step factor, and due to impurities of standards used in the addition procedure.
14
Contamination:
The estimates of percent contamination are listed
in Table 2, The average percent total contamination is about four
and a half percent.
However, it is very important to notice that
in at least ten of the sphenes nearly all of the contaminating
material was quartz.
One would expect quartz to contribute very
little to the contamination in the elements being analysed for.
This is especially true when quartz is compared to minerals such
as augite, hornblende, or hematite. Hematite for instance containa seventy percent iron, and a twenty milligram sample with a
one percent contamination by hematite would have 7000 ppm of iron
due to the hematite alone.
This is very considerable contamination
and is an extrem example.
Hematite is quite unlikely to be
present as a result of the separation procedure used.
Most con-
taminating materials will contain many times less of the contaminating elements than hematite contains iron.
Quartz can be
expected to make essentially no significant contribution to the
contamination of the semple in any of the analysis elements.
On
the basis of this consideration and the observation of ten samples, whose only visually detectable granular contamination was
quartz, the estimated average effective contamination is about
22
0
two and a half percent.
This lies well within the error introduced
by the analyst.
2.
plate Develoment:
7Errors due to development are extremnely smsll
on the same plate.
TrIrors from plate to plate due to variations
in the plates and in the development of each plate are thought to
have been largely compensated for by calibrating each plate in
three separate wavelength regions and by the use of comparison
standards on each plete.
Mrror due to this source is considered
to be negligible in relation to errors introduced by the analytical procedure,
3. ?rror due to Non-linear Step Factor:
As explained earlier, a
step sector with an assumed linear step factor of one-half and
later one-fourth derived from the g sometry of the sector was ueed
during the invostigation,
Actually, however, the intensity of the
light in the are varies with the position in the are gap, and thus
the intensity of the light reaching different steps on the sector
varies (sen Dennen, 1949),
In order to minitize the error from
thia source, intensity readings were made on the same stop wherever
possible.
However, this was not possible in many cases and thus
since the factors of one-half or one-fourth were assumed, error
has resulted.
Based on the work of Dennen (1949, illustrated in
figure 11 of his manuscript) concerning this problem, light from
the center of the are was as accurately as possible caused to fall
along the slit.
Dennen found that the intensity in the central
portion of the are was the most nearly constant.
In this way it
is felt that the error from this source was minimized.
It has
been assumed in this investigation that this source has not
23
contrIbuted eignificnntly to the error,
4. Error2 due to lpurity of Standards Useod:
elen~ats
Oxides of the analysis
t Teprepnring the additton standrds are in generRal
quite pure and contributn errors which are very definitey negligiblo, and actually in most cases lie
below the detection limit.
This is the case for the oxides of zirconum, iron, yttrium,
vanadium, tungsten, chromium and scandium used in this study.
(The oxides are listed in Table 3.)
rare-earths, it
Rowever, in the case of the
is much more probable that larger errors, signifi-
cant ones perhaps, may have been introduced due to impurity of the
oxides used in preparing the stendards.
The reasons for this lie
basically in the great nimilarity of the various rare-earth elements and thus the greater ease with vhich they substitute for
one another.,
The kind or degree of contnxmination of the rare-
earth oxides used is not known.
however.
It is known that they nre old,
It is felt that error from this
oiwoe, especially in
the cases of samarIum and gadolinium may be real,
Wit since no
date is available on the nurity of these oxides, it was not possible to make any corrections and it was assumed that only the
analysis eleent of the oxide was present.
In the second group are errors introduced in weighing and mixing of
additive oxidesloading and arcing of the samples, measurement of line intensity, construction of curves and errors due to loss of unvolatilized
samples
1. Weighing irrors:
All weighings of the additive oxides were made
to the nearest tentit of a milligram.
rror due to this source is
certainly considerably less than a percent.
2.
Mixing Yrrors:
Mrrors due to non-uniform mixing of the oxide
eAddtive is untknown.
The mixing roceAdure described ;asrlier is
conidered to hrm rerAered error tron tM.- sou:c to be nlw
i-
cIble.
3,
%ror due to Loading and A'ircing of the Sprles:
From twelve
lofided electrodes used in the addition mocedure it
is es:timated
that the error in the sarple weighta sroed is of the order of
five percent.
This Varetion in sample weights, of course, Is
also reeponsible in
and thus exposure.
about
P
come measure for variation in sroing tire
As mentioned earlier the arcing time showed
five percent voriation elsa.
The nature of the relation-
ship between sample weight eid aroinr tine is not knotn, and was
rot investigated in this study.
Eowever, somr
indicetion of a
relttonshlp between variations in san-le 'eight
and aeiri
time
ray be seen in figure 1.
4.
2Wrors due to Measuremeont of Line and Enckgrotud Intensittes:
?rrore firm this source are, fror reneral erperience in the Cabot
Lraboratory at Y.I.T. where this work ras carried out, considered
to be of the order of one percent.
5. Error# due to Loss of Unvoletilized Sample:
Errors due to this
souree are unknown, but considered to be small, leas than s percent,
The
raing conditions and weight ratio of sphene to carbon
used gave a very steady end smooth arc, with very little sputtering.
None of the samples used in the analysis had any significant
noticeable sample loss.
All semples were areed to completion.
6. Errors due to Construction and Use of Curves:
Errors from this
source can be introduced at three stages in the particular
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procedure used in this investigation. Errors are introduced in
the plotting of the addition curves used to determine the original
amiount of each element present in Sphene 3085.
These curves also
introduce error efter plotting, in the interpoletion to determine
the original concentrntions of the various elements.
This problem
is discussed under the section deaJing specificlly with the addition procedure.
Tt is sufficient here to note thnt errors in
this part of the study '411 here en imnportant effect on determine.
tions in all the saM'oltes, stince it
the concentrations in al
is by the standard (3035) that
the rest of the semples are determined.
The sfftct will be a shift of all determinations in the same
dtire'ction frrom- somw aRolute v'ue,
A second rlaco where errors 3re inrtoduced th-ough graphical
procedures is in the plotting and the use of calibr9tion curves.
This error, w.hile pronbl
not an
,ritirO or as generalized in
effect as the error involved in the eddition plots, could be
ocalif
ant.
It
ia sfilt, howeviir,
ie to the construction of
rmny such curves, that the slopo of these uirrea is subject to a
comparativaly sanll arror.
The reywaining graphical orror is thtt involved wi
ing curves Cor each elensat.
the work-
Thie also is disicussed in more de-
tail *lSewhereB.
No aotual oatimate of the error du
use of theoe ourvta
is available.
to the construction and
Uowever, it
seems reasonable
to expect that an error of fru rive to ten pereent &ay be introduced from this uoarce.
------------
.............
.
It is estimated that the total probable error involved in the determinations reported lies between about ten percent to perhaps as much as
twenty percent.
error.
Different elements will have somewhat different probable
While these sound like, and are, sizeable errors that need to be
allowed for, it is important to realize that the importance say of a
twenty percent error quantitatively speaking is dependent on the general
level of concentration of the particular element.
Thus with a 100 ppm
level of concentration similar to the values obtained for chromium, the
actual value lies between 80 and 120 ppm. While in a
case such as iron
with a general level of about 20,000 ppm, the possible values range between 16,000 and 24,000 ppm,
28
ANALYTICAL PROUD(DURE
Method of Analysis
In order to make quantitative measurement of the elements of interest,
it is necessary to construct a "yardstiek" using one of the samples.
this has been done, this standard an
Once
be used to make determinations of
these same elements in the rest of the samples.
I chose
the standard aine it contained no visible impurities.
sample 3085 as
The addition
method was employed to detemine the original concentrations of the
analysis element a in sphene 3085.
In this method an oxide mix containing equel or nearly equal amounts
by weight of each of the fourteen original analysis elements was prepared.
A list of the sources of these analysis elements and the percentage of the
source that is made up by the analysis element is given in Table 3. This
oxide mix was then mixed with sphene 3085 in such a proportion that each
analysis element had an approximate concentration of one percent or 10,000
ppm. Then one part of this prepared addition sample was mixed with nine
parts of pure sphene 5085.
This gave an approximate concentration of about
1000 ppm in each of the analysis elements.
In analagous fashion other ad-
dition concentrations of 5,000, 2,500, 350, 100 and 35 ppm were prepared.
After mixing these samples one part to two parts of carbon by weight, they
were arced in duplicate.
Addition plots were then prepared to determine
the original concentration of the analysis elements in the pure sphone
3085.
The graphical procedure is discussed in the section concerning ad-
dition plots.
29
Table 3
Compounds of the fourteen original analysis elements used in
the addition procedure and the percent of each comprised by
the analysis element
Campound
Percent of
Analysis
Element
Ce20 3
85.A ce
La203
85.3 La
Gd(N0 3 ) 3
45.8 ad
Nd2 0 3
85.7 Nd
V2 0 5
56.0 V
Y20 3
78.8 Y
Mn02
63.2 Mn
MoO 3
66.7 Mo
w
100.0 W
ZrO2
71.0 Zr
Cr20 3
68.4 Cr
Fe20 3
69.9 Fe
Sc20 3
65.3 So
Sm
100.0 Sm
-
4' aN
I--
0.11
A
ft , W
I 1
i9i
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Graphical Procedure
Three types of plots were used to determine the concentrations of the
analysis elements. These are calibration curves, addition plots and working curves,
Calibration 'urves: A calibration curve has to be used at each wavelength in order to convert defleetions from the miorophotometer to relative
intensities.
slopes.
Calibration curves for different lines may have different
A separate calibration curve was prepared for each line listed in
Table 1 on the addition part of this investigation, which was all contained
on one photographic plate.
Examiuation of these curves showed that only
three calibration curves were required.
One was for use with molybdenum
3903, a second used for manganese 4031 and 4034, and the third was used for
a
0
the region 4200 A to 4500 A, which region included the rest of the analysis
lines.
Addition Plots:
Two plotting techniques were used for each analysis
line in the addition part of the procedure.
The first of these was the
standard addition plot discussed in Ahrens (1955, page 33).
This is merely
a plot of the relative intensity of the line of an element as the ordinant
versus the amount of the element added to the sample, on the aboissa,
curve is then drawn through a succession of these points.
A
Ideally this is
a straight line which is then extended to intersect the aboissa.
The point
of intersection of the aboissa and the extended addition curve indicates
the original concentration of the analysis element in the sample,
The second type of plot is the same in all respects except that the
intensity of the analysis line was ratioed to the intensity of one of the
major element lines, calcium or titanium.
These mjor elements were
assmed to be present in an essentially constant proportion,
This method
then is really just the internal standard method applied to the
addition
plot,
To the best of the author's tnowledge the only previous use of this
ratio
teethod
with addition plots, "we that of Ahrens and Gorfinkle (1951),
In this article little more was said of the method other than steting the
fact of its use.
In the particular case of this investigation, calcium, camprising
about twenty percent of sphene was used as the constant internal standard
element for all analysis elements except chromium and zirconium.
calcium line used was 4302.
The
In the cases of chromium and zirconim,
titanium, making up about twenty-five percent of sphene was used.
Since
there does seem to be some relation between the weight of sample and areing time, there is presumably some effect also on the measured intensity
of the lines,
It was hoped that by using this ratio of intensities, that
variation in the sample weight in the addition procedure would be compensated for and result in addition plots whose points would be the same
as if there had been no variation in sample weight.
It is important to note here, as concerns the graphical procedure,
that while both of these types of addit ion plots ideally give a straight
line, this is not the case in actual experimental work.
One important
suspected cause of the non-linearity of the addition plots, is that as the
concentration of the analysis element increases, the amount of self-absorption also increases.
This of
course varies with the element. This would
have the effect of reducing the intensity of the line at higher concentrations and thus result in a decrease in the slope of the addition plot at
these higher concentrations.
This decrease of the slope of the addition
curve with increasing concentration of the analysis *lement, especially
at the 10,000 ppm added level, was noted in all oases except twv or three
of the ratioed addition plots. In nearly all oases the ratioing of intensities is observed to have reduced the amount of non-linearity as compared to that of the ordinary plots.
In constructing the addition plots and determining the original concentrations in aphene 3065, the straight line that best £ittea the curve
defined by the lower concentration points () through 5000 ppm added) was
used.
It does not sem that the ratioing of the intenaity of the analysis
line to that of the calcium or titanium line necessarily reduces the variation of the two points from the mean,
However, the ratioed type of ad-
dition plot definitely does seem to increase the linearity of the addition
curve in many oases,
This definite improvement is illustrated in figures
2 and 3, which show the results for iron 485 and iron 4E60.
As can be
seen from the figures both iron lines give larger values for the original
iron concentration in sphsne 3085, in the standard addition plot, than
they do in the ratioed addition plots.
Also in eaoh case the linearity of
the ratioed addition curve is increased over that of the standard curve.
This is particularly evidenced in the case of iron 4383, in which case a
straight line can be drawn entirely within the envelope of intensity ratio
variation at all points of concentration.
This ratioed addition ourve
determination of iron was used as the experimentally determined iron content of sphene 3085.
I have drawn as can be seen in figure 3 the best
curve through the ratioed intensity points for iron 4260, which gives
nearly the same value obtained from the ratioed iron 4383.
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In Mst cases the ratioing did seem to give improved values.
There
were some ceses, however, in which the ratioing did not improve the curve
at all and may in a case or two have made it worse.
Working
urves:
After determining the concetration of the variouc
analyaia elements irL the
andard, working curves were establishedc
constructed fur each element.
on each plate.
and
A working curve was plotted for ea:h element
This was done by plotting points fror three different known
concentration levels of the standard for each element on each nlate,
iflope of the working curve for each element
degre$s (Ahruns, 1951).
The
as assmed to be forty-five
The base experimentail working curve eqas conatructed
from the addition data, using all the concentration levels prepred. In
most oases the conoontration determined from the addition plots gave a
working curve with a slope of nearly forty-five degrees and thus agreed
quite well the asamed slope suggested by Ahrena.
In the ease of chroa itum,
yttrium and gadolinlia, minor adjustments were made in the original concentrations of these elements in sphene 3085, until the working ourve was
within a degree or two of forty-five degrees.
this adjustment is as follows.
The exact procedure used in
When the angle of the working ourve is
nuch greater than forty-five degrees, the original concentration used for
the working curve was too high, while an angle less than forty-five degroes indicates that the original concentration used was too low.*
This
procedure was used in detail with manganese, which is discussed below.
In the case of mngenene, two analysis lines, Vn 4031 and Mn 4034,
were chosen for purposes of furnishing a check throughout the invostigetion.
The original concentration of manganese in aphene 3085 as determined
*Personal communication from Dr. W. H. Dennen.
from the best addition plots, was 4700 ppm from Mn 4031 and 3800 ppm from
Un 4034, For both lines all the working ourves for all the plates used
were plotted for each of the two assumed original concentrations in aphene
3085.
In all oases exoept the working curve from the addition material
for Mn 4031, the angles of the curves for the 4700 ppm coneentration were
considerably greater than forty-five degrees. On the basis of the above
mentioned criteria the 4700 ppm value was regarded as being too large.
The angles of the working curves for the 3800 ppm concentration were in
all except the case of the addition plot for Mn 4031, very close to fortyfive degrees.
Thus 3800 ppm was the concentration value used for manganese
in pure sphene 3085.
In the determinations of the analysis elemntiats from the working curves,
only one line of each element was used.
Selection of the line used in each
case was based on considerations of apparent sensitivity (as revealed by
the addition plate) and aininwa interference.
general method of selection was manganese,
The only exception to this
In the ease of eanganese, the
working curves indicated that Mdn 4034 gave more reliable intensity values
for the remaining twenty-two samples.
Thus, for these samples, intensity
values for tn 4034 were used in preference to those of An 4031. The
analysis lines used in the final working curve stage were:
Fe 4385
A
MA 4034
Y 4398 A
Sm 4329 A
Gd 42522
V
4379 A
Ce 4222 A
Or 4254 A
Zr 4239 A
Nd 4303 A
S
4374
La 4335 A
W 4294 A
Molybdenun was discarded as an analysis element in this $tage, when it was
found that overcompensation had occurred for every sample when a correction
factor was applied,
ISCUSSION OF RSILTS
The concentrations of each analysis element in each sample are tabulatod in Table 4.
'eeh
value shown in the table is in all cases, except a
few, the average of two determinations.
Also given in Table 4 is the
average peroent deviation from the mean or probable error for each element,
This figure was calculated for each element by dividing the deviation from
the mean of each pair of determinations, by the raean itself, and then
totaling all these deviations and dividing by the total number of samples
for which two quantitative determinations were made.
oxpressed in percent.
This answer was then
Thus in the case of chromium the average percent
deviation from the mean is 6,76 percent.
This means that any reported de-
termination for chromium has a fifty percent chance of being within 6,76
percent of the correct value.
The error of the averge of twc determna-
tions is then simply the probable error of L single determtination divided
by the aquare root of'two,
i.a., 6,78 /VW
for chromium.
possible to make quantitative deteriminations in all cases.
It was not
In these oases
the elements were not detected or at best just gave trace indications.
The beat that could be done was to take a rough estimate of the neximum
pos-ible concentration.
This was done in all cases exoopt one for
tungsteu and numerous times in the case of siandium.
Th
avsrag~e of thu two determiations for each elenent of each sample
are plotted both. by clemant, graphs 1-,
and by sample, graphs 10-%.
Smi-
Lgarithnic paper has ber used in the plots in order to accommodate the
wide differencue in conxentrtlon, emd vntain raative variations of the
elements.
semplea.
The results wll first te discussed by element end then by
Table 4
Average Concentration of Analysis Elements in Each Sample
(All vaue ,given in parts per million)
Sample Fe
Mn
Y
V
or
4383 4034
4398 4379
3011
8250
5200
16001o0101360
3055
9300
1930
2320
Zr
c
La
Nd [
W
Gd
4239 42221 433 4303 4329
O262
137 4294
680 500 340 27201 165011650 140
8601600
1000
490
470 2450 1220 1390
3014
21350 615o 11400 470
28
4450
550
530
2120 4900 5000 510
3058
i615o
3650
3720 1080
70
490
200
260
1400 2100 2050 130
410o
7850
220
28
52o
320
275
1910 5800 3950 <75
22000
650 165 2250
820
450 3780 9450 5800 980
3071
20350
3080
27500
4620
3139
24000
5320
3051
24200
6400
3060
21100
5950
3061
3062
4120 300
475
ND
ND
ND
ND
18 2280 1360 1660 2500 3020 2950 130
ND
750 1160 520
2680 7800 5900 '75
78
580 1620
950
4050 4500 4000 360
ND
20400 3900,
63o0 860 100
2o800 1030
700
1750 5700 3900 280
ND
18250
5300
3640
760 31
2350 4250 4020
8350 3980 1980 160
ND)
rae
3063, 18150
4780
"4100 1060
67
2800 4020 2180
8500 6500 3850 210
3079
22300
4050
880
85
3081
20750
2760
3082
3485
18250
14850 440 26
600
9550
1365o
820 4780 1780 11200 5450 3700 380
3700 570 125
3120 3600 2290
6100 3650 2080 <75
20800 3350
2420
130
1900 148o 1330
1880 1700 1100
2680
1860
860 91 2380 8150 3980 10350 5250 2060 475
2120
310 36
22
00
ND
5900 3580 3550
4950 2600 3820 <75
730
ND
99511040 23 390012850 2680
4550 1450 2420 100
ND
92 1760 3820 2280 5150 2000 1500 210
ND
3100 4200 3000
4200 1850 1800 150
WD
2180
3067
21950
5170
3069
15500
2750
3084
13000
620
3085
15900
3800
2700
800
2093
1165
19140
2480
9140 635
820 8700
1550 2020 1650 '75
3013
15250
8550 15500 240 38 18900 100 100
970 2200 COO
3138
51500 I1750
_10
ND
ND
NI
ND
740 1060
ho0
70
1160 16
14_37 1 3v03 15
33
2280 1340 1000 <s;&
3480 2600 180
178 14.4415642791LJ.78J3.01385 1 7651
* overcorrected for iron conflict
E-.not detected, less than 200 ppm
Discussion o
1.
Resot
Iron:
b
Element
Iron (graph 1) is present in all samples.
The iron content
varies from about 8,000 to 28,000 ppm, with the exception of over
51,000 ppm in sample 3136.
It is almost a certainty that much of
this last value is due to contamination, as indicated by the eztimated trelve percent contemination consisting of opaque grtins
(Table ?).
Most of the iron values seem to lie in the neighbor-
hood of 20,000 ppm.
On* can notice some degree of
imilarity in
the shpe of the Curves for gedolinium (graph S), sameriuam
(graph 7),
and iron*
2, Chromium:
0hromium (graph 1) to clso present in all samples,
Chromium values en much more vsriable prnportionately than iron
ard
rer
grent deel lower,
lees ter ?00 ppm.
The
All the semples tnalysed contrtned
erjoritr o+f the Yrlu- , e
may be asen
from either Table 4 or graph 1, are less than 100 per.
It
is
noticed that the three samplee containing the highest
eoncentre-
tions of chrorium also have the three loest
These
.
sanples are 3055,
Manenrtese:
Mangenese
moat of the
3011 end P,091
(gryph
vslies of iron.
4
1) is nroesnt in all
a'mpos, with
lvalues lying in the range of 4000 to 6000 ppm,
There
zmeerrs to be "eneral eimilsrity in the sbaps of the crvtes ffor
manganese (graph 1) and gadolinlum (grenh 8),
Zironirm:
afsnrien.
Zirconium (graph 2) was found to be prsent in all
The variability in concentration is rather high.
half of the values obtained lie between 1800 and 3000 ppm.
About
An
unusually high conoentration of almost 19,000 ppm is reported for
sample 3013.
It
rould seem likely that some of this is due to
77
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5. Vanadium:
Vanadium (graph 3) was found in all samples and varies
from about a 100 ppm to about 1200 ppm.
Most of the samples had
values between 800 and 1200 ppm.
6. Yttrium:
Yttrium (graph 4) showe a wide range of variation from
about 700 ppm to about 22,000 ppm and is present in all samples.
Most of the values lie in the range 3500 to 6800 ppm. It is po.
sible that a few of the very high values may in part be due to
contamination as all samples with high values have at least three
percent contamination.
7. Lanthanum:
Lanthanum (graph 5) was found to be highly variable
in concentration and was present in all samples,
teept for a few
extreme oases the values lie between 300 and 4000 ppm.
Lanthanum
generally seas to have values which are the inverse of yttrium,
i.e., in general when a sample has a low yttrium concentration,
the lanthanum value is reasonably high and vice versa.
As may be
seen from graphs 5 and 6, there is a definite parallelism of the
ooneentrations of lanthanum, cerium and neodymium.
When a sample
is low in one of these elaments it is also low in the other two.
8.
Cerium:
Cerium (graph 5) was found in all samples and was highly
variable in oonentration.
The values determined ranged from
about 100 ppm to about 8000 ppm. There seems in general to be an
inverse relationship between eerium and yttrium values,
9.
Neodymium:
Neodymium (graph 6) varies over a range of 130 ppm to
about 11,000 ppm, and was found to be present in all samples except two, which is discussed below.
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As mentioned earlier Nd 4303 has a conflict with an iron line
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that part of the intensity of this lino due to iron, the following procedure was followed.
A samiple containing a mixture of ferric oxide and quartza
arced,
was
Then the ratio of the intensities of Fe 4303 to Pe 4383
was calculated.
Since the F 4383 intensity was known for each
sample, it then became theoretically possible to coalulate how
much of the intensity of the line at 4303 was due to iron.
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theoretically leaving just the intensity due to the neodymium
present.
In all cases except two this procedure gave positive intensity
values, which are meaningful.
However, in the ases of samples
3013 and 3138, negative intensity values resulted,
This certainly
indicates that these samples were quite low in neodymium relative
to the other samples, and it has been assumed in this study that
they were also low in absolute concentration.
The negative in--
tensity values, which have no real meaning, do indicate that there
is some sort of an inaccuracy in the correction factor used.
It
would seem that there has been some overcorreotion to give these
negative values.
Thus it is probable that all the samples have
been somewhat overoorrected#
Since most of the samples already
have high neodymium values, the elimination of this overcorrect ion
would simply increase the peaks for this element seen in the sample
plots.
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neodymium, while reasonably high, does not constitute a peak, but
might become a peak value in these sample plots if not overcompensated.
Thie would eliminate one of the more common discrepancies
noted in the discussion of results by samples,
However, both 3013
and 3138 would still be low in neodymium relatively speaking,
10.
Samarium:
Samarium (graph 7) wae found to be present in all san-
plea and varies from ap proximately 1000 to almost 10,000 ppm.
In
all except two or three eases, the concentrations of samarium and
gadolinium (graph 8) parallel each other.
In addition to the gen-
eral parallelism observed in graphs 7 and 8, one notices that the
actual conentrations of each of the elements are in many oases
similar numerically.
11.
Gadolinium (graph 8), like samarium, was present in
Gadolinium:
all samples and varies over a range of 1100 ppm to about 6000 ppm#
12.
Scandium:
samples.
Scandium (graph 9) was not detected in seven of the
It is estimated that the concentration of scandium in
these samples is 75 ppm or less.
A trace amount of scandium was
detected in three other samples and are tabulated as having values
near 100 ppm.
The remaining samples have values varying from 130
to almost 980 ppm.
13,
Tungsten:
Tungsten was detected in only two samples,
The non-
detection is estimated as indicating that lese than 200 ppm of
the element is present in the sample.
Semi-quantitative estimates have been made for strontium and aluminum.
The strontium estimates were made using line Sr 4215.5 and the aluminum
estimates were made from line Al 3961.5.
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other samples showed any detectable strontium.
A.
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of the samples eon-
tained aluminua, estimated to be present in quantities of 10,000 to 20,QQ
ppm in each sample.
Diaoussion of Results
Q
Sample
In this presentation and discussion of the date by samples, I am
attempting to determine by trace element analysis if any of the sphenes
might be from genetically related rooks.
Reasonable evidence of genetic
similarity or relationship between two sphenes and also presumably between
the two rock sources from which they were separated, is taken to be a
parallel relationship between the plots of the concentration of the elements in each of the two samples.
It seems reasonable to expect that two
*phenes from genetically related rocks would illustrate similar relations
between elements.
It seems well to point out here that there may not
always be complete agreement or similarity due to the errors involved in
the determinations, but that a general similarity is necessary.
If two
samples have nearly the same concentration of the elements, one might
suspect they came from not only from genetically related sources, but that
the sources were also in close geographical proximity,
The samples are discussed by groups erranged on the basis of the
author's impression of significant similarity end relationship,
The only
relationship among the samplesof the last group is that they have little
or no similarity to any other samples in the author's opinion,
In the first group are samples 3011, 3014, 3051, 3055, 3058, 3060,
3061, 3062, 3063, 3071, 5079, 3080, and 3139.
In general these samples
have high peak concentrations in yttrium, iron, neodymium, samarium, and
gadolinium.
Samarium is usually higher than gadolinium.
These samples
also have minimum values for scanuium, lanthanum, dhromium and tungsten.
Cerium is often nearly as low as lanthanum.
Closer similarity between
some of the semples than between others was noted within the group.
The
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group.
The first subgroup of group one contains samples 3011 and 3055 (graph
10).
plea.
There appear
to be two distinguishing characteristics of these same.
First, both have decidedly higher chromium values and decidedly
lower iron values than any of the other samples in this group.
Second,
the peak concentrations, while agreeing with the general case for the
group as far as elements are concerned, are considerably lower than the
concentrations of the same elements in the rest of the samples of group
one.
This Is especially noticeable in the cases of yttrium and iron,
In
the case of iron both of these samples have less than 10,000 ppm, while the
rest of the samples all have at least 16,000 ppm,
The second subgroup of group one contains samples 3014, 3058, 3071,
3080, and 3139 (graphs 11 and 12),
These samples are distinguished from
the other samples except those in subgroup one on the basis of their cerium
values, which are nearly as low as the lanthanum values and in the cases of
3058 and 3139 are somewhat lower.
quality.
The first subgroup also possesses this
The second subgroup was separated from the first on the observa-
tion that in subgroup to
the samarium and gadolinium values are in all
cases greater than the values for neodymium, -while in subgroup one the
neodymium values are in all cases greater than both the samarium and
gadolinium values.
Sample 3014 (graph 11) shows a dissimilarity, with a
peak concentration for zirconium.
Thie, if not a real variation, could
be due to too large a zirconium value or too small a neodymium value,
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might be due to contamination by some zircon, as we notice from Table 2.
that this sample has an estimated nine percent contamination.
It should
also be noted that the scandium values in aamplea 3014 and 3080 (graph 12)
are higher than in most samples of this group,
The third subgroup of group one contains samples 3051, 3060, and 3061
(graph 13).
This subgroup differs from the first two in that the cerium
values are substantially higher then the lanthanum values.
This subgroup
differs from the fourth and last subgroup in that the samarium and
gadolinium concentrations are substantially larger than the neodymium concentration.
Sample 3061 has an apparent discrepancy in a peak value for
zirconium, which may be due in part to contamination.
This is not neces-
sarily true, as it can be seen from graph 2 that this value for zirconium
is in the general range of zirconium values.
The fourth subgroup of group one contains samples 3062, 3063, and 3079
(graph 14).
This subgroup differs from the first two, in that it does not
have a minima for cerium.
It differs from the third subgroup by virtue of
the fact that samariua and gadolinium values are lower in each sample than
the neodymium value.
In the case of sample 3062, the lanthanum value does
not show a minima or low point, but was determined to be slightly greater
than samarium. This is the only discrepancy within this subgroup, and it
can be seen that if this lanthanum value (4000 ppm) were lowered by twentyfive percent this discrepancy would be eliminated.
This percent change is
not too much greater than the estimated ten to twenty percent possible
error.
It may well be that this relatively high lanthanum value is due to
contamination.
The estimated nine percent contamination could conceivably
account for an additional 2000 ppm of lanthanm above that normally present
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in the sphene.
Sample 3062 has been included in this subgroup after the
above consideration and on the observation of definite similarity in the
cases of all other elements.
Actually, samples 3062 and 3063 not only
show a parallel relationship, but in all elements except three, they show
nearly equal conoentration levels, As can be seen from the map of sample
locations these two samples are within about five miles of each other.
The above mentioned observation about the similar quantities of the
analysis elements present would seem to indicate that the rocks from
which these samples came are very closely related. They may be from the
same igneous body.
The second group contains samples 3081, 3082 and 3485 (graph 15).
This group like the first group has peaks for iron, neodymium, samarium
and yttrium.
There are minimas for chromium, scandium and tungsten.
This
second group differs from the first group in that the zirconium, neodymium,
cerium and lanthanum values all are greater than the gadolinium values for
their respective samples,
Also the lanthanum is rauch higher relative to
samarium in this group than is the case in the first group.
Sample 3082
is slightly out of phase by its lack of a peak for neodymium.
The third group contains samples 3067 and 3069 (graph 16).
Here again
chromium, scandium and tungsten are lov and iron is high. Other general
patterns present in the other groups are changed.
Cerium and lanthanum,
while not attaining peak values, are quite high relatively.
are not low values.
They certainly
Also the samarium concentrations in both oases are
significantly lower (about 1000 ppm) than the gadolinium values.
It should
be noted that these samples show different relations as regards zirconiumneodymium and vanadium-yttrium. However, their general similarity otherwise
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The fourth group contains samples 3084 and 3085 (graph 17).
This
group differs in the occurrences of minima within the group of elements
samarium and gadolinium.
The
lowest value in both samples is found to be thrt for gadolinium.
This
zirconium, noodymiw,
cerium, lanthenum,
value is not overly low in relation to most of the 'bove mentioned eleThe similarity between these two samples could be more striking,
ments.
Sample 3084 has peek values for neodymium and vanadium, which 3085 does
not.
It would be possible with an adjustment or two for each sample in
group three and group four, to bring the curves of these samples into general similarity with the samples of group two.
no justification or reason for doing so.
The author, however, sees
In samples 3084 and 3085, for
instance, a decrease of 400 to 800 ppm in the samarium concentration would
bring these two samples into similarity with samples 3067 and 3069.
In the fifth group are samples 2093, 3013 and 3138 (graphs 18, 19,
and 20).
The samples of this group show no overall similarity either to
each other or to any of the other samples.
The zirconium value of nearly
19,000 ppm in sample 3013 is thought to be due in pert to contamination,
This value is about 13,000 ppm higher than the next highest zirconium
value, Sample 3013 is also notable for its very low values for neodymium,
cerium and lanthanum,
Saml
3138 (graph 20) is similar to the samples in group one with one
very striking exception, namely a very low neodymium value.
However, it
should also be noted that this sample has an extremely high value for iron,
over 51,000 ppm.
This is more than 20,000 ppm greater then the next highest
iron value for any of the other samples.
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It
is quite probable that a 'major portion of this value Is due to
contamination, estimated to be about twelve percent, a.l of whioh consists
of opaque grains.
The problai of overaoApensation in the correction of
the neodymium line was discussed earlier, However, it is possible that
the overoompensation was unduly severe here due to the exceptionally high
iron value., It is, of course, impossible to know if 5138 would show any
greater similarity to group one if this overcompensation was eliminated.
Sumary
of.
Results
and
Conclusions
Results indicate that sphenes are generally low (up to several hundred
ppm) in ohrorium, scandium and tungsten.
Elerients present in the middle
range of concentretions from about 1000 to 3500 ppm, include lanthanum,
ceritm, gadolirium, samarium, zirconium and vanadium.
Present in somewhat
higher concentrations are mangenese, yttrium ani neodymium.
All the above
elements were only occasionally present in quantities greater than a per-
cent.
Iron values are very much higher then any of the other elements
studies, averaging about two percent.
This is as might be expected due to
the greater geochemical abundance of iron as compared to the other elements.
A portion of this high value for iron doubtless is due to contamination,
Aluminum, while not determined quantitatively, is estimated to be present
in the range of one to two percent.
There very definitely appears to be parallelism between the values of
lanthanum, cerium and neodymium present in sphene.
of these elements is also high in the other two.
also shoi very striking parallelism.
pected from considerations of
A sample high in one
Samarium and gadolinium
These relations are as might be ex-
ionic radii (see Table 5),
An inverse re-
lation is noted between iron and chromium in cases of highest chromium or
lowest iron values.
Lanthanum and cerium show an inverse relationship
with yttrium.
Of the thirteen samples of group one, chosen as having significant
similarities b y the author, eleven are from New England, end two are trom
Quebec.
Of the eleven from New Rngland, three are from Massachusetts out
of four samples from that state, and eight are from Maine of nine samples
from there. The only Maine sample not listed in group one is the standard
I
low
00"
Table 5
Tabulation of Ionic Radii of Certain Elements
Element Valence Radius
in
Element
Valance
OA
Radius
in
OA
Ca
+2
1.06
Ti
+4
0.64
Y
+3
1.06
Al
+3
0.57
La
Ce
1.22
Cr
+3
0.65
Nd
Gd
+3
+3
+3
1.18
1.17
Fe
Fe
+2
+3
0.83
0.67
+3
1.11
SM
Mnn
+3
+2
1.13
0.91
V
V
Mo
+3
+4
+4
0.75
0.61
0.66
Sr
+2
1.27
Mo
+6
0.62
U
Th
+4
+4
1.05
W
+4
0.68
1.10
Si
+4
0.39
(From Appendix
Stillwell, 1938 and The Handbook of
PThysics and Chemistry)
The locations of the samples eroqpt for 3485, in far western Ontario,
3085.
ean be seen on the map of sample looalities (figure 4).
two, 3031, 3082, and 3485 are ell from Onterio.
The samples of group
Samples 3081 end 3082 are
within ten miles of each other, while 3485 is about eight hundred miles
Sinilarity is also noted between semples 3067 and 3069, which also
away.
show some geographicel proximity.
The remainder of the samples show rela-
tively little truce element similarity and no geographical relationship.
There thus does appear to be some definite geographical grouping of the
samples, with New England being by far the most obvious group.
The reason
other geographically groupings are not so obvious may well be due to the
much fewer number of samxplea from these areas.
The grouping of samples by similarity of their plots for the thirteen
analysis elements, vould seem to indicate that trace element analysis of
sphenes can be used, given enough samples from an area, in correlating
rocks that have some genetic and geographical relationship.
It is possible
that this is due only to the general selective nature of sphenes, selecting
the various elements in certain proportions to each other in nearly all
cases.
It would seem, though, f rom ti
fact that only little more than
half the samples (group one) show general similarities amongst themselves,
while the rest seem to be signifioantly dissimilar from this group, that
there is soma genetic relationaship indicated.
The author concludes that
trace element analysis of aphenes may be helpful in establishing due fact
of genetic relationship between rocks.
Of course, additional work is
necesaary, as will be suggested briefly under recommendations for future
work,
It is concladed with respect to procedure, that the use of intensity
ratios of an analysis element with a similarly behaving element present in
ryure
4.
p
of SaPmpi/e
Lo ca/ities
nearly constant proportion in additionplcts is quite helpftd.
It
was
found in this investigation that this intensity ratio in ILost orses ixm4r more neerlxy linear and thus making
proved the addition plot E,
9 making thm
it easier to
<etermine
ment s in the stanidard,
the original concertrations of the analysis ele-
The use of tuese ratios for thi
prpose is recom-
mended.
: tatulation of elements and their concentration runges in sphene by
various analysts is presented in Pable 6,
Table 6
Elements and their Concentration Ranges in Sphene
by Various Analysts
(All values given in
Oxide of
Element
19p03
3"Shaa
(1946 )
0-19,100
parts per million)
Rose
(1959)
Prince
(1938)
Element
9500-61,700
Fe
8250-27,500
Zr
500-5900
0-10,700
FeO
1000-6900
Zro
2
500-1100
cr 2 0 3
100-200
Cr
15-635
La 2 0 3
200-500
La
100-8700
Ce2 03
600-1900
0o
100-8150
200-9600
2203
Y
740-22,000
Nd 2 0 3
600-800
Nd
500-11,200
Od2 0 3
100-300
Gd
1100-5900
SagO3
100-300
Sa
970-9450
MAO
100-800
Un
620-8550
v
130-1160
v
200-750
V205
1100
35,800
0-500
50-1100
30203
300
So
75-980
A120 3
0-44,400
Al
10,000-20,000
Sr
1200-2600
SrO
40-4400
tNb205
300-16,000
Ta206
100-1?,500
Pr2 0 3
0-200
Ob
(1)500-10,000
Dy205
0-200
U
(2) 25-1270
r205
G-00
Th
(2)
Yb203
0-100
(1) Taffe (1947)
(2) Hurley and Pairbairn (1957)
TT
40-3150
I ...........
i................
- - -1--1.
I
I
, 0
1
A '
-
-
I
Recorennations for ?uture Work
Analysis of the rocks tron shioh
elents
tuld furnis
roA and spho
permit.
It
z4amples of sphene came for major
usefufl information.
Petrogrcphic stuzdies of the
would Ulso be helpful if tine and purposes of the study
vould be very helpful in an investigation of the type reported
in this thesis to oheek the detemnhat ions of ecl element by a different
oethod, ooectlily for thi
standardl.
Quantitetive deterninations in the
ztanaard are the ones needing the iost verification,
are used to determine the values in other samples.
oince these values
The above ouggestions
for additional work would furnish greater confidence and reassurance in
the result s obtained and thus also in the interpretationsmade.
However, more important purposes wauld be served by analysing additional aphene samples and establishing greater geographical density of
trace elements analyses for the mineral, especiafly in areas from which
few aphenes have been analysed.
In order to draw any really well based
conclusions concerning the topio of this thesis it is necessary to have a
statistically significant number of analyses.
Idven
more significant and indicative would be a similar trace element
analysis of several accessory minerals from each of the rock samples.
If
several mineral phases indicated that certain rocks appeared to be genetieally related, one would be much more confident in his conclusions.
23LiOGURAIy
269
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80